反应详情

温度

65 °C

A stirred mixture of 7-acetyl-5-chloroquinolin-8-yl trifluoromethanesulfonate (0.12 g, 0.34 mmol, from Example 47, Step 2), 1-cyclobutylpiperazine dihydrochloride (0.087 g, 0.41 mmol), palladium acetate (1.5 mg, 0.0068 mmol), (S)-(−)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (6.3 mg, 0.010 mmol), and cesium carbonate (0.44 g, 1.4 mmol) in tetrahydrofuran (3 mL) was heated at 65° C. overnight. The mixture was cooled, diluted with dichloromethane and filtered. The filtrate was washed with brine, dried over MgSO4 and and evaporated to dryness. The residue was purified on silica gel (eluting with 0 to 10% methanol in dichloromethane) to give the desired product (69.2 mg, 59%). LCMS calculated for C19H23ClN3O (M+H)+: m/z 344.2; Found: 344.1

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washThe filtrate was washed with brine
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customThe residue was purified on silica gel (eluting with 0 to 10% methanol in dichloromethane)